An advanced hydrothermal modification method was developed to synthesis Ni/Al2O3 catalyst with perfect activity. SEM, XRD, DTA-TG and XPS were used to characterize the textural properties of the materials obtained after each synthesis step. The experimental results indicated that the modification of the impregnation samples at elevated temperatures enhanced the absorption of Ni(NO3)(2)(.)xH(2)O on the surface of supporters which were composed mainly of Al(OH)(3) and AlOOH, leading to the formation of the porous sintering products (NiAl2O4/Al2O3) with bigger specific surface areas and higher Ni contents. The conversion of CH4 increased a lot by using the hydrothermal-modified catalyst instead of using the catalyst prepared via the traditional impregnation-sintering route. (C) 2004 Elsevier B.V. All rights reserved.